Quote from https://wiki.dmt-nexus.m...ss_NaOH.2C_Salts.2C_Etc. :



Let's say we only bring the pH down to 8.0.

According to Infundibulum's calculator, only 1.56% harmaline and 66.6% harmine is in freebase form at pH 8.0.
So such a cleanup will remove pretty much all harmaline, and a third of the harmine.

The point of bringing the pH up is to freebase more alks. If we are to bring the pH back down to 8 in the cleanup stage, what's the point of *ever* increasing it above 8 in the basification stage? Any alks we gain by upping the pH from X to Y, we lose by bringing it back from Y to X.

Why not just base until we've reached pH 8.0 and stop there? Our yield will be poor, but the cleanup would make it equally poor anyway.

I must clearly be missing something here?

I cant say for sure because my understanding of the mechanics of how insoluble substances effect PH is limited, but it seems to me that washing with cold distilled water you should have a PH of around 7 if all base is washed out. I am assuming that without the prescense of a dissolved acid the harmalas will be almost completely insoluble in cold water & the PH of 8 may be due to fine particles of harmine/harmaline suspended in the liquid.

I could be entirely wrong here & washes could be eating huge amounts of yeilds, but it works to yeild a usable product at the very least.

There is a solution if you do not like washing. You should be able to base, filter, dissolve the filtrate in acetic acid & then just manske to purify, dissolve the HCL salts in minimal amount of water, base using minimal amounts of ex. 1 mole NaOH solution, filter, manske, etc.

Thanks. So that would mean the less vinegar used in the extraction, the less sodium acetate in the basic solution and the less loss of yield by washing?

Also it would mean the freebase / salt percentages given by the calculator are not absolutes and depend on other factors. According to the calc, over 95% harmaline should be in salt form at pH 8.5. But if the solution is only distilled water + sodium carb, and there is no acetic acid (as sodium acetate) or any other acid in it, 0% harmaline is in salt form as there is no acid for it to bind to. So in that case, the calculator is off by 95 percentage points.

If you think you are losing yeild in washing why not try taking your wash water & basing it to see if anything precipitates?

I appologize for not being able to offer a more scientific approach but the scope of my knowledge here is very limited. Im am fairly confident that if the washes were negatively impacting yeild in a large way or were somehow chemically not sound some of the more knowledgable members here would have made it a point to correct the information & explain how to do things the right way.

If further understanding of the mechanics behind washing freebase harmalas in water is what you seek you might try asking around in chat. There are certainly some members here who can answer your question in great detail.

Mind that the calculator is a strict theoretical thing.

You will perceive a mist on your bottom. Been there. Question is how much did you loose by washing.

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First you base high to obtain max alkaloids.
Then you wash and loose some alkaloids.

Jagube, that is not the same as basing not high (say eight) and retrieving a very poor amounts of alkaloids that you don't need to wash anymore. Then again you don't need to wash of the base , yes indeed, but you still need to wash of the soup out of which it was filtered.

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* I've been giving the hint before: in your last basing step use sodcarb saturated water to base the alkaloids with. Filter them. Do only 1 or 2 washes with water on your precips and done with. Traces of sodcarb is no problem, and it's my experience that the crystals stay better white than those obtained by lye-basing and a ton of water-washing to remove the lye.

* If you final end-base with lye, you can then do several washes with sodcarb water so that will hold your harmaline safe, wash 100x if you want. Then wash 1 x with plain water. To make sodcarb wash water, only a pinch in a bottle is enough to elevate pH to not loose the harmaline.

* make ammonia wash water, it will keep the pH up and high so you wont loose harmaline and once drying all the ammonia goes away. A 3% ammonia liquid is fine for such purposes. If you want minimal ammonia, drip some in your wash water and as soon as you have pH 9 or 10 then stop adding ammonia, now you have least ammonia present.


There are possibilities

The washes are done so that you don’t consume NaOH.
In my experience, caapi extracted alkaloids are insoluble in pH neutral water.

That makes sense, there's little harmaline to loose with caapi.

Yes that's exactly what I do in harmala extraction. Several washes with cold distilled water until the supernatant water is somewhat clear. It does not seem to lower the yield.

Even better, use vacuum filtration and wash the filter. This has an advatange of cleaning and drying the freebase at the same time.

You can also use sodium carbonate for final basing instead of lye, that is more "food safe" so to say. Not sure if that will work for caapi, but certainly works for rue.